CN107501921A - A kind of composition of modified fiberglass reinforced PA 6 and preparation method thereof - Google Patents
A kind of composition of modified fiberglass reinforced PA 6 and preparation method thereof Download PDFInfo
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- CN107501921A CN107501921A CN201610426010.0A CN201610426010A CN107501921A CN 107501921 A CN107501921 A CN 107501921A CN 201610426010 A CN201610426010 A CN 201610426010A CN 107501921 A CN107501921 A CN 107501921A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The present invention provides a kind of modified composition of fiberglass reinforced PA 6 and preparation method thereof, and it is by 30 60 parts of PA6,1 10 parts of PA12,25 45 parts of glass fibres, 5 15 parts of magnesium sulfate crystal whiskers, 05 parts of toughener, 5 10 portions of nucleators and 5 10 parts of surface modifiers are blended, extruding pelletization is prepared.The present invention is cooperated by magnesium sulfate crystal whisker and surface modifier, improve the bond state between glass and nylon resin, reduce the separation of glass and nylon resin, glass is set to be coated well in nylon resin, glass flowing synchronous with resin in process, it is not easy to rip, greatly reduces the exposed of glass.And improve the mechanical performance and compressive property of the modified composition of fiberglass reinforced PA 6.
Description
Technical field
The invention belongs to field of polymer composite material, and in particular to a kind of modified composition of fiberglass reinforced PA 6 and its system
Preparation Method.
Background technology
Polyamide (PA, being commonly called as nylon) is that DuPont develops resin for fiber at first, real in nineteen thirty-nine
Now industrialize.Polyamide starts to develop and produce injection-molded item the 1950s, meets downstream industry system with substituted metal
The low requirement of product lightweight, cost；In addition, PA has a good combination property, including mechanical property, heat resistance, wear resistance,
Chemical proofing and self lubricity, and coefficient of friction is low, it is easy to process also with certain anti-flammability.
Currently in order to strengthening PA6 toughness and reducing its production cost, appropriate glass is mostly added inside nylon material
Fibre is modified to it, but adds after glass and then easily occur floating fine phenomenon.It is usually to be caused by glass emergence on the surface to float fine phenomenon,
White glass floats during plastic melt filling flow and is exposed to appearance, is just formed after shaping to be condensed on plastic surface radial
White vestige, can be more obvious because shade deviation increases when plastic is dark colour such as black.So float fine phenomenon not only shadow
The cosmetic look of PA products is rung, has an effect on its performance as resistance to rolled-up stock.
The content of the invention
It is an object of the invention to provide a kind of modified composition of fiberglass reinforced PA 6 and preparation method thereof, improve outside glass
The phenomenon of dew.
Technical scheme is as follows：
A kind of composition of modified fiberglass reinforced PA 6, it is prepared by weight by following components：
Further scheme, the intrinsic viscosity range of the PA6 is 0.6-1.0dl/g.
The glass fibre is short glass fiber, and its length is 2-5mm, a diameter of 7-13 microns.
The average grain diameter of the magnesium sulfate crystal whisker is 100 μm, compression strength 100Mpa, density 0.25g/cc.
The toughener is selected from maleic anhydride grafted ethene-octene copolymer, ethylene-methyl acrylate copolymer or second
One or more in alkene-methyl acrylate-GMA.
The nucleator is sodium benzoate.
The surface modifier is the mixture of modified ethylene bis-fatty acid amides (TAF) and silicone, wherein modified ethylene
The minimum addition of bis-fatty acid amides is 2 parts.
Another goal of the invention of the present invention is to provide the preparation method of the above-mentioned composition of modified fiberglass reinforced PA 6, and it is walked
It is rapid as follows：
(1) PA6 and PA12 are dried respectively；
(2) by proportioning, by dried PA6 and PA12, and glass fibre, magnesium sulfate crystal whisker, toughener, nucleator and
Surface modifier, add in high-speed mixer stir 3-5min together；
(3) well mixed material is added from the charge door of double screw extruder, through double screw extruder melting extrusion,
It is granulated, is prepared into the modified composition of fiberglass reinforced PA 6.
PA6 is to dry 4-5h under the conditions of temperature is 110-140 DEG C in the step (1)；It in temperature is 110- that PA12, which is,
4-5h is dried under the conditions of 120 DEG C；
220-250 DEG C of the area's temperature of double screw extruder one, two 225-265 DEG C of area's temperature, three area's temperature in the step (3)
235-275 DEG C, four 245-285 DEG C of area's temperature, five 240-280 DEG C of area's temperature, six 245-285 DEG C of area's temperature, head temperature 245-
285 DEG C, engine speed is 15-35HZ.
The present invention compared with the existing technology, has the advantages that：
1st, TAF is to introduce polar group on the basis of ethylene bis-fatty acid amides in surface modifier, and it is mixed with silicone
Its compatibility between glass fibre is enhanced after conjunction；TAF solvation segment has certain intermiscibility with matrix resin,
This TAF has played phase solvent.So, surface modifier and magnesium sulfate crystal whisker cooperate, glass fibre, basic resin it
Between form similar anchoring node, i.e. crosslinking points, improve the bond state of glass and resin, reduce point of glass and resin
From.
2nd, due to the mechanical function thickness degree increase between the surface of glass and matrix resin, make to be in glass near surface
Matrix be easier to occur shear yielding, increase the absorption to impact energy and dissipative effect, promote glass between matrix resin
Toughening effect.So that glass is coated well in resin, glass flowing synchronous with resin in process, no
Easily rip, greatly reduce the exposed of glass.
3rd, surface modifier and magnesium sulfate crystal whisker cooperate and reduce glass emergence on the surface, so as to correspondingly reduce glass
With the friction of screw rod, the moment of torsion of screw rod is set also to decrease, it is easy to process.
4th, PA12 has higher fusing point, and it can also keep stronger strength and stiffness in higher temperature, so in the present invention
PA12 is added to improve the mechanical strength of PA6 compositions.
5th, the composition of modification fiberglass reinforced PA 6 prepared by the present invention has excellent mechanical property.
Embodiment
The present invention is further illustrated with reference to embodiments.
Measuring mechanical property method：
Composition prepared by the present invention is molded into test examination using injection molding machine of plastic using GB standards at 230-270 DEG C
Sample, the size (length x width x thickness) of its test bars are respectively：Tensile bars (dumbbell shape), 170.0 × 10.0 ×
4.0；Bending batten, 80.0 × 10.0 × 4.0；Non-notch impact batten, 80.0 × 10.0 × 4.0；Notch shock batten, 80.0
× 10.0 × 4.0, v-notch, notch depth 1/5.
In temperature be (23 ± 2) DEG C, in the standard environment that humidity is (50 ± 5) % after placement 16h after test bars shaping
Tested, test environment is (23 ± 2) DEG C, humidity is (50 ± 5) %.
Tensile strength and elongation at break：Tested by GB 1040, draw speed 5mm/min.
Bending strength and bending modulus：Tested by GB 9341, rate of bending 1.25mm/min.
Simply supported beam notch impact strength：Tested by GB 1043.
Glass fiber content：Tested by GB 9345.
Embodiment 1
(1) by PA6 in 110 DEG C of temperature, dry 4h；PA12 is in 110 DEG C of temperature, dry 4h；
(2) weigh dry 60 parts of PA6,1 part of PA12,25 parts of glass fibre, 5 parts of magnesium sulfate crystal whisker, 5 parts
Sodium benzoate, 5 parts of surface modifier (mixture of 2 parts of modified ethylene bis-fatty acid amides and 3 parts of silicone)；
(3) material weighed up in above-mentioned steps (2) is stirred into 3min in high-speed mixer；
(4) charge door of double screw extruder and then by above-mentioned well mixed material is added；
(5) material is granulated through double screw extruder melting extrusion；
The processing technology of described double screw extruder is：230 DEG C of one area's temperature of double screw extruder, two area's temperature 245
DEG C, three 255 DEG C of area's temperature, four 265 DEG C of area's temperature, five 260 DEG C of area's temperature, six 265 DEG C of area's temperature, 265 DEG C of head temperature, main frame
Rotating speed is 15HZ.The performance test results are shown in Table 1.
Embodiment 2
(1) by PA6 in 140 DEG C of temperature, dry 5h；PA12 is in 120 DEG C of temperature, dry 5h；
(2) weigh 40 parts dry of PA6,10 parts of PA12,30 parts of glass fibre, 5 parts of magnesium sulfate crystal whisker, 5 parts
Toughener maleic anhydride grafted ethene-octene copolymer, 10 parts of sodium benzoate, 8 parts of surface modifier (3 parts of modified second
Support the mixture of bis-fatty acid amides and 5 parts of silicone)；
(3) material weighed up in above-mentioned steps (2) is stirred into 5min in high-speed mixer；
(4) charge door of double screw extruder and then by above-mentioned well mixed material is added；
(5) material is granulated through double screw extruder melting extrusion；
The processing technology of described double screw extruder is：220 DEG C of one area's temperature of double screw extruder, two area's temperature 225
DEG C, three 235 DEG C of area's temperature, four 245 DEG C of area's temperature, five 240 DEG C of area's temperature, six 245 DEG C of area's temperature, 245 DEG C of head temperature, main frame
Rotating speed is 35HZ.The performance test results are shown in Table 1.
Embodiment 3
(1) by PA6 in 120 DEG C of temperature, dry 5h；PA12 is in 120 DEG C of temperature, dry 5h；
(2) weigh 40 parts dry of PA6,5 parts of PA12,35 parts of glass fibre, 10 parts of magnesium sulfate crystal whisker, 3 parts
Toughener ethylene-methyl acrylate copolymer, 2 parts of ethylene-methyl acrylate-glyceryl methacrylates, 8 parts of benzene
Sodium formate, 10 parts of surface modifier (mixture of 5 parts of modified ethylene bis-fatty acid amides and 5 parts of silicone)；
(3) material weighed up in above-mentioned steps (2) is stirred into 5min in high-speed mixer；
(4) charge door of double screw extruder and then by above-mentioned well mixed material is added；
(5) material is granulated through double screw extruder melting extrusion；
The processing technology of described double screw extruder is：240 DEG C of one area's temperature of double screw extruder, two area's temperature 255
DEG C, three 265 DEG C of area's temperature, four 275 DEG C of area's temperature, five 270 DEG C of area's temperature, six 275 DEG C of area's temperature, 275 DEG C of head temperature, main frame
Rotating speed is 35HZ.The performance test results are shown in Table 1.
Embodiment 4
(1) by PA6 in 140 DEG C of temperature, dry 5h；PA12 is in 120 DEG C of temperature, dry 5h；
(2) weigh 30 parts dry of PA6,5 parts of PA12,45 parts of glass fibre, 10 parts of magnesium sulfate crystal whisker, 5 parts
Sodium benzoate, 5 parts of surface modifier (mixture of 2 parts of modified ethylene bis-fatty acid amides and 3 parts of silicone)；
(3) material weighed up in above-mentioned steps (2) is stirred into 5min in high-speed mixer；
(4) charge door of double screw extruder and then by above-mentioned well mixed material is added；
(5) material is granulated through double screw extruder melting extrusion；
The processing technology of described double screw extruder is：250 DEG C of one area's temperature of double screw extruder, two area's temperature 265
DEG C, three 275 DEG C of area's temperature, four 285 DEG C of area's temperature, five 280 DEG C of area's temperature, six 285 DEG C of area's temperature, 285 DEG C of head temperature, main frame
Rotating speed is 35HZ.The performance test results are shown in Table 1.
Comparative example 1
(1) by PA6 in 110 DEG C of temperature, dry 4h；PA12 is in 110 DEG C of temperature, dry 4h；
(2) 50 parts dry of PA6,5 parts of PA12,35 parts of glass fibre, 5 parts of toughener maleic anhydride is weighed to connect
Branch ethylene-octene copolymer, 5 parts of sodium benzoate；
(3) material weighed up in above-mentioned steps (2) is stirred into 3min in high-speed mixer；
(4) charge door of double screw extruder and then by above-mentioned well mixed material is added；
(5) material is granulated through double screw extruder melting extrusion；
The processing technology of described double screw extruder is：220 DEG C of one area's temperature of double screw extruder, two area's temperature 225
DEG C, three 235 DEG C of area's temperature, four 245 DEG C of area's temperature, five 240 DEG C of area's temperature, six 245 DEG C of area's temperature, 245 DEG C of head temperature, main frame
Rotating speed is 15HZ.The performance test results are shown in Table 1.
Comparative example 2
(1) by PA6 in 110 DEG C of temperature, dry 4h；PA12 is in 110 DEG C of temperature, dry 4h；
(2) weigh 40 parts dry of PA6,5 parts of PA12,35 parts of glass fibre, 10 parts of magnesium sulfate crystal whisker, 5 parts
Toughener maleic anhydride grafted ethene-octene copolymer, 5 parts of sodium benzoate；
(3) material weighed up in above-mentioned steps (2) is stirred into 3min in high-speed mixer；
(4) charge door of double screw extruder and then by above-mentioned well mixed material is added；
(5) material is granulated through double screw extruder melting extrusion；
The processing technology of described double screw extruder is：220 DEG C of one area's temperature of double screw extruder, two area's temperature 225
DEG C, three 235 DEG C of area's temperature, four 245 DEG C of area's temperature, five 240 DEG C of area's temperature, six 245 DEG C of area's temperature, 245 DEG C of head temperature, main frame
Rotating speed is 15HZ.The performance test results are shown in Table 1.
Comparative example 3
(1) by PA6 in 110 DEG C of temperature, dry 4h；PA12 is in 110 DEG C of temperature, dry 4h；
(2) 40 parts dry of PA6,5 parts of PA12,35 parts of glass fibre, 5 parts of toughener maleic anhydride is weighed to connect
Branch ethylene-octene copolymer, 5 parts of sodium benzoate；
(3) material weighed up in above-mentioned steps (2) is stirred into 3-5min in high-speed mixer；
(4) charge door of double screw extruder and then by above-mentioned well mixed material is added；
(5) material is granulated through double screw extruder melting extrusion；
The processing technology of described double screw extruder is：220 DEG C of one area's temperature of double screw extruder, two area's temperature 225
DEG C, three 235 DEG C of area's temperature, four 245 DEG C of area's temperature, five 240 DEG C of area's temperature, six 245 DEG C of area's temperature, 245 DEG C of head temperature, main frame
Rotating speed is 15HZ.The performance test results are shown in Table 1.
Table 1
Embodiment can be seen that modified fiberglass reinforced PA 6 produced by the present invention with the comparison of comparative example and combine from upper table 1
The bending modulus of thing, tensile strength, elongation at break, simply supported beam notch impact strength are obviously higher than material prepared by comparative example
Material, and article surface is bright, without floating fibre.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using this hair
It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to implementation here
Example, for those skilled in the art according to the announcement of the present invention, not departing from improvement that scope made and modification all should be
Within protection scope of the present invention.
Claims (9)
- A kind of 1. composition of modified fiberglass reinforced PA 6, it is characterised in that：It is prepared by weight by following components：PA6 30-60 parts,PA12 1-10 parts,Glass fibre 25-45 parts,Magnesium sulfate crystal whisker 5-15 parts,Toughener 0-5 parts,Nucleator 5-10 parts,Surface modifier 5-10 parts.
- A kind of 2. modified composition of fiberglass reinforced PA 6 according to claim 1, it is characterised in that：The characteristic of the PA6 is glued Degree scope is 0.6-1.0 dl/g.
- A kind of 3. modified composition of fiberglass reinforced PA 6 according to claim 1, it is characterised in that：The glass fibre is Short glass fiber, its length are 2-5mm, a diameter of 7-13 microns.
- A kind of 4. modified composition of fiberglass reinforced PA 6 according to claim 1, it is characterised in that：The magnesium sulfate crystal whisker Average grain diameter be 100 μm, compression strength 100Mpa, density 0.25g/cc.
- A kind of 5. modified composition of fiberglass reinforced PA 6 according to claim 1, it is characterised in that：The toughener is selected from Maleic anhydride grafted ethene-octene copolymer, ethylene-methyl acrylate copolymer or ethylene-methyl acrylate-methacrylic acid One or more in ethylene oxidic ester.
- A kind of 6. modified composition of fiberglass reinforced PA 6 according to claim 1, it is characterised in that：The nucleator is benzene Sodium formate.
- A kind of 7. modified composition of fiberglass reinforced PA 6 according to claim 1, it is characterised in that：The surface modifier To be modified the mixture of ethylene bis-fatty acid amides and silicone, wherein the minimum addition of modified ethylene bis-fatty acid amides is 2 Part.
- 8. a kind of preparation method of composition of modification fiberglass reinforced PA 6 as described in claim any one of 1-7, its feature exist In：Its step is as follows：（1）PA6 and PA12 are dried respectively；（2）By proportioning, by dried PA6 and PA12, and glass fibre, magnesium sulfate crystal whisker, toughener, nucleator and surface Modifying agent, add in high-speed mixer stir 3-5min together；（3）Well mixed material is added from the charge door of double screw extruder, through double screw extruder melting extrusion, made Grain, is prepared into the modified composition of fiberglass reinforced PA 6.
- 9. preparation method according to claim 8, it is characterised in that：The step（1）It in temperature is 110- that middle PA6, which is, 4-5h is dried under the conditions of 140 DEG C；PA12 is to dry 4-5h under the conditions of temperature is 110-120 DEG C；The step（3）Middle 220-250 DEG C of the area's temperature of double screw extruder one, two 225-265 DEG C of area's temperature, three area temperature 235- 275 DEG C, four 245-285 DEG C of area's temperature, five 240-280 DEG C of area's temperature, six 245-285 DEG C of area's temperature, head temperature 245-285 DEG C, engine speed is 15-35HZ.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110172243A (en) * | 2019-06-20 | 2019-08-27 | 横店集团得邦工程塑料有限公司 | A kind of modified Pa 6 of low water absorption/PA12 alloy material and preparation method |
| CN111138855A (en) * | 2020-01-08 | 2020-05-12 | 柳州塑友科技有限公司 | Modified nylon material for automobile bumper |
| CN111892813A (en) * | 2020-07-28 | 2020-11-06 | 横店集团得邦工程塑料有限公司 | Low-odor reinforced toughened flame-retardant PA6 composite material and preparation method thereof |
| CN111909510A (en) * | 2020-08-11 | 2020-11-10 | 广东聚邦兴材科技有限公司 | Nylon composite material and preparation method thereof |
| CN114672070A (en) * | 2022-03-15 | 2022-06-28 | 上海金发科技发展有限公司 | Modified glass fiber and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104231616A (en) * | 2013-06-07 | 2014-12-24 | 上海杰事杰新材料(集团)股份有限公司 | Reinforcing toughening high-temperature-resistant nylon composite material and preparation method thereof |
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- 2016-06-14 CN CN201610426010.0A patent/CN107501921A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104231616A (en) * | 2013-06-07 | 2014-12-24 | 上海杰事杰新材料(集团)股份有限公司 | Reinforcing toughening high-temperature-resistant nylon composite material and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110172243A (en) * | 2019-06-20 | 2019-08-27 | 横店集团得邦工程塑料有限公司 | A kind of modified Pa 6 of low water absorption/PA12 alloy material and preparation method |
| CN111138855A (en) * | 2020-01-08 | 2020-05-12 | 柳州塑友科技有限公司 | Modified nylon material for automobile bumper |
| CN111892813A (en) * | 2020-07-28 | 2020-11-06 | 横店集团得邦工程塑料有限公司 | Low-odor reinforced toughened flame-retardant PA6 composite material and preparation method thereof |
| CN111892813B (en) * | 2020-07-28 | 2023-01-10 | 横店集团得邦工程塑料有限公司 | Low-odor reinforced toughened flame-retardant PA6 composite material and preparation method thereof |
| CN111909510A (en) * | 2020-08-11 | 2020-11-10 | 广东聚邦兴材科技有限公司 | Nylon composite material and preparation method thereof |
| CN114672070A (en) * | 2022-03-15 | 2022-06-28 | 上海金发科技发展有限公司 | Modified glass fiber and preparation method and application thereof |
| CN114672070B (en) * | 2022-03-15 | 2023-08-29 | 上海金发科技发展有限公司 | Modified glass fiber and preparation method and application thereof |
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